#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:27:44 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180040 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/34/7033473.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7033473
loop_
_publ_author_name
'Fernandes, Tiago A.'
'Solařová, Hana'
'Císařová, Ivana'
'Uhlík, Filip'
'Štícha, Martin'
'Štěpnička, Petr'
_publ_section_title
;
 Synthesis of phosphinoferrocene amides and thioamides from carbamoyl
 chlorides and the structural chemistry of Group 11 metal complexes with
 these mixed-donor ligands.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3092
_journal_page_last               3108
_journal_paper_doi               10.1039/c4dt03279a
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C48 H44 Ag Fe2 N2 O2 P2, Cl O4, C H Cl3'
_chemical_formula_sum            'C49 H45 Ag Cl4 Fe2 N2 O6 P2'
_chemical_formula_weight         1181.18
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-10-16 deposited with the CCDC.
2014-12-23 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 91.9850(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   18.0426(3)
_cell_length_b                   14.5715(2)
_cell_length_c                   9.2242(2)
_cell_measurement_reflns_used    8073
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      2.26
_cell_volume                     2423.66(7)
_computing_cell_refinement       'SAINT V8.27B (Bruker AXS Inc., 2012)'
_computing_data_collection       'Bruker Instrument Service v2012.12.0.0'
_computing_data_reduction        'SAINT V8.27B (Bruker AXS Inc., 2012)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0216
_diffrn_reflns_av_sigmaI/netI    0.0284
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            12514
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    1.328
_exptl_absorpt_correction_T_max  0.856
_exptl_absorpt_correction_T_min  0.747
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1196
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.767
_refine_diff_density_min         -0.766
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.045(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         4906
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0258
_refine_ls_R_factor_gt           0.0242
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0236P)²+2.5686P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0529
_refine_ls_wR_factor_ref         0.0538
_reflns_number_gt                4751
_reflns_number_total             4906
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt03279a2.cif
_cod_data_source_block           tf20
_cod_depositor_comments
'Adding full bibliography for 7033464--7033475.cif.'
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               7033473
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Ag Ag 0.0000 0.431311(12) 0.5000 0.01847(7) Uani 1 2 d S
Fe Fe 0.155460(19) 0.32573(3) 0.21028(4) 0.01945(9) Uani 1 1 d .
P P 0.12598(3) 0.48415(5) 0.46943(7) 0.01754(14) Uani 1 1 d .
O O -0.03991(10) 0.30174(14) 0.3436(2) 0.0290(5) Uani 1 1 d .
N N -0.02078(13) 0.15904(16) 0.2606(3) 0.0265(5) Uani 1 1 d .
H1N H -0.0011 0.1221 0.2002 0.032 Uiso 1 1 d R
C1 C 0.04975(14) 0.28222(19) 0.1637(3) 0.0203(5) Uani 1 1 d .
C2 C 0.10140(16) 0.2302(2) 0.0832(3) 0.0304(7) Uani 1 1 d .
H2 H 0.1082 0.1656 0.0876 0.036 Uiso 1 1 calc R
C3 C 0.14032(18) 0.2916(3) -0.0036(3) 0.0441(9) Uani 1 1 d .
H3 H 0.1783 0.2753 -0.0676 0.053 Uiso 1 1 calc R
C4 C 0.11391(19) 0.3811(3) 0.0198(3) 0.0438(9) Uani 1 1 d .
H4 H 0.1306 0.4352 -0.0263 0.053 Uiso 1 1 calc R
C5 C 0.05792(15) 0.3764(2) 0.1246(3) 0.0282(6) Uani 1 1 d .
H5 H 0.0309 0.4267 0.1617 0.034 Uiso 1 1 calc R
C6 C 0.18414(13) 0.39914(18) 0.3908(3) 0.0185(5) Uani 1 1 d .
C7 C 0.17825(14) 0.30356(18) 0.4243(3) 0.0212(5) Uani 1 1 d .
H7 H 0.1456 0.2771 0.4913 0.025 Uiso 1 1 calc R
C8 C 0.22971(16) 0.2551(2) 0.3399(3) 0.0267(6) Uani 1 1 d .
H8 H 0.2375 0.1906 0.3405 0.032 Uiso 1 1 calc R
C9 C 0.26748(14) 0.3199(2) 0.2544(3) 0.0269(6) Uani 1 1 d .
H9 H 0.3050 0.3061 0.1879 0.032 Uiso 1 1 calc R
C10 C 0.24009(13) 0.40857(19) 0.2845(3) 0.0229(6) Uani 1 1 d .
H10 H 0.2558 0.4644 0.2422 0.027 Uiso 1 1 calc R
C11 C -0.00649(14) 0.24905(18) 0.2646(3) 0.0198(5) Uani 1 1 d .
C12 C 0.17507(14) 0.51492(18) 0.6393(3) 0.0223(6) Uani 1 1 d .
C13 C 0.24412(18) 0.4789(2) 0.6818(3) 0.0329(7) Uani 1 1 d .
H13 H 0.2684 0.4376 0.6194 0.039 Uiso 1 1 calc R
C14 C 0.2777(2) 0.5026(2) 0.8142(4) 0.0442(9) Uani 1 1 d .
H14 H 0.3245 0.4773 0.8423 0.053 Uiso 1 1 calc R
C15 C 0.2433(2) 0.5624(3) 0.9044(3) 0.0480(10) Uani 1 1 d .
H15 H 0.2665 0.5785 0.9949 0.058 Uiso 1 1 calc R
C16 C 0.1751(2) 0.5997(2) 0.8648(3) 0.0455(9) Uani 1 1 d .
H16 H 0.1516 0.6416 0.9275 0.055 Uiso 1 1 calc R
C17 C 0.14103(17) 0.5756(2) 0.7321(3) 0.0340(7) Uani 1 1 d .
H17 H 0.0940 0.6009 0.7051 0.041 Uiso 1 1 calc R
C18 C 0.13631(14) 0.58612(18) 0.3569(3) 0.0201(5) Uani 1 1 d .
C19 C 0.20165(15) 0.63716(19) 0.3585(3) 0.0241(6) Uani 1 1 d .
H19 H 0.2432 0.6174 0.4163 0.029 Uiso 1 1 calc R
C20 C 0.20648(17) 0.7168(2) 0.2761(3) 0.0294(6) Uani 1 1 d .
H20 H 0.2512 0.7512 0.2776 0.035 Uiso 1 1 calc R
C21 C 0.14601(19) 0.7457(2) 0.1919(3) 0.0345(7) Uani 1 1 d .
H21 H 0.1493 0.8001 0.1359 0.041 Uiso 1 1 calc R
C22 C 0.08106(18) 0.6961(2) 0.1887(3) 0.0332(7) Uani 1 1 d .
H22 H 0.0397 0.7163 0.1307 0.040 Uiso 1 1 calc R
C23 C 0.07608(16) 0.6165(2) 0.2705(3) 0.0264(6) Uani 1 1 d .
H23 H 0.0312 0.5824 0.2676 0.032 Uiso 1 1 calc R
C24 C -0.07935(18) 0.1197(2) 0.3438(4) 0.0411(8) Uani 1 1 d .
H24A H -0.0671 0.1266 0.4475 0.062 Uiso 1 1 calc R
H24B H -0.0846 0.0544 0.3201 0.062 Uiso 1 1 calc R
H24C H -0.1261 0.1514 0.3200 0.062 Uiso 1 1 calc R
C1S C 0.0000 0.8625(4) 0.5000 0.0666(19) Uani 1 2 d S
H1S H -0.0088 0.9001 0.5885 0.080 Uiso 0.50 1 d PR
Cl1S Cl 0.05505(10) 0.93185(15) 0.3962(2) 0.0554(4) Uani 0.50 1 d P
Cl2S Cl 0.06428(11) 0.76758(18) 0.5668(2) 0.0558(4) Uani 0.50 1 d P
Cl3S Cl -0.07796(10) 0.82782(18) 0.4514(2) 0.0558(4) Uani 0.50 1 d P
Cl1A Cl 0.00403(13) 0.94796(9) 1.03522(13) 0.0359(4) Uani 0.50 1 d P
O1A O -0.0346(3) 1.0240(3) 0.9695(6) 0.0512(13) Uani 0.50 1 d P
O3A O -0.0394(5) 0.8731(4) 1.0432(11) 0.090(3) Uani 0.50 1 d P
O2A O 0.0688(4) 0.9272(8) 0.9491(8) 0.102(3) Uani 0.50 1 d P
O4A O 0.0313(3) 0.9749(4) 1.1762(5) 0.0504(13) Uani 0.50 1 d P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
P Ag P 142.99(3) 2_556 .
P Ag O 93.16(5) 2_556 .
P Ag O 115.50(4) . .
P Ag O 115.50(4) 2_556 2_556
P Ag O 93.16(5) . 2_556
O Ag O 80.19(10) . 2_556
C7 Fe C6 41.29(11) . .
C7 Fe C1 108.16(10) . .
C6 Fe C1 123.07(10) . .
C7 Fe C5 125.25(11) . .
C6 Fe C5 108.57(11) . .
C1 Fe C5 40.94(11) . .
C7 Fe C8 40.84(10) . .
C6 Fe C8 69.04(11) . .
C1 Fe C8 123.75(12) . .
C5 Fe C8 161.37(11) . .
C7 Fe C3 156.42(14) . .
C6 Fe C3 160.29(13) . .
C1 Fe C3 68.20(11) . .
C5 Fe C3 68.28(14) . .
C8 Fe C3 120.34(14) . .
C7 Fe C2 121.72(12) . .
C6 Fe C2 158.61(11) . .
C1 Fe C2 40.94(11) . .
C5 Fe C2 68.71(12) . .
C8 Fe C2 106.40(13) . .
C3 Fe C2 40.18(13) . .
C7 Fe C10 69.16(11) . .
C6 Fe C10 41.30(9) . .
C1 Fe C10 159.18(11) . .
C5 Fe C10 122.65(11) . .
C8 Fe C10 68.57(12) . .
C3 Fe C10 122.70(11) . .
C2 Fe C10 158.28(10) . .
C7 Fe C9 68.59(11) . .
C6 Fe C9 68.74(10) . .
C1 Fe C9 159.51(12) . .
C5 Fe C9 157.27(12) . .
C8 Fe C9 40.61(12) . .
C3 Fe C9 106.23(12) . .
C2 Fe C9 122.22(12) . .
C10 Fe C9 40.39(11) . .
C7 Fe C4 162.16(14) . .
C6 Fe C4 124.76(14) . .
C1 Fe C4 68.34(11) . .
C5 Fe C4 40.71(12) . .
C8 Fe C4 155.81(13) . .
C3 Fe C4 40.22(15) . .
C2 Fe C4 67.92(14) . .
C10 Fe C4 107.52(12) . .
C9 Fe C4 120.98(12) . .
C6 P C18 105.04(12) . .
C6 P C12 104.07(12) . .
C18 P C12 103.40(12) . .
C6 P Ag 113.06(8) . .
C18 P Ag 116.03(9) . .
C12 P Ag 113.97(8) . .
C11 O Ag 133.18(17) . .
C11 N C24 121.2(2) . .
C11 N H1N 123.3 . .
C24 N H1N 114.9 . .
C5 C1 C2 107.7(2) . .
C5 C1 C11 123.5(2) . .
C2 C1 C11 128.8(3) . .
C5 C1 Fe 69.57(15) . .
C2 C1 Fe 69.68(15) . .
C11 C1 Fe 128.66(18) . .
C3 C2 C1 107.8(3) . .
C3 C2 Fe 69.83(17) . .
C1 C2 Fe 69.37(15) . .
C3 C2 H2 126.1 . .
C1 C2 H2 126.1 . .
Fe C2 H2 126.3 . .
C2 C3 C4 108.9(3) . .
C2 C3 Fe 69.99(16) . .
C4 C3 Fe 70.19(18) . .
C2 C3 H3 125.5 . .
C4 C3 H3 125.5 . .
Fe C3 H3 125.9 . .
C3 C4 C5 108.1(3) . .
C3 C4 Fe 69.59(19) . .
C5 C4 Fe 69.30(16) . .
C3 C4 H4 125.9 . .
C5 C4 H4 125.9 . .
Fe C4 H4 126.8 . .
C4 C5 C1 107.4(3) . .
C4 C5 Fe 69.99(17) . .
C1 C5 Fe 69.50(15) . .
C4 C5 H5 126.3 . .
C1 C5 H5 126.3 . .
Fe C5 H5 125.8 . .
C7 C6 C10 107.4(2) . .
C7 C6 P 122.42(18) . .
C10 C6 P 130.1(2) . .
C7 C6 Fe 69.25(14) . .
C10 C6 Fe 69.90(14) . .
P C6 Fe 124.02(13) . .
C8 C7 C6 108.1(2) . .
C8 C7 Fe 70.12(15) . .
C6 C7 Fe 69.46(15) . .
C8 C7 H7 125.9 . .
C6 C7 H7 125.9 . .
Fe C7 H7 126.1 . .
C9 C8 C7 108.0(3) . .
C9 C8 Fe 69.96(16) . .
C7 C8 Fe 69.04(16) . .
C9 C8 H8 126.0 . .
C7 C8 H8 126.0 . .
Fe C8 H8 126.6 . .
C10 C9 C8 108.7(2) . .
C10 C9 Fe 69.66(15) . .
C8 C9 Fe 69.43(16) . .
C10 C9 H9 125.6 . .
C8 C9 H9 125.6 . .
Fe C9 H9 126.8 . .
C9 C10 C6 107.8(2) . .
C9 C10 Fe 69.95(15) . .
C6 C10 Fe 68.80(14) . .
C9 C10 H10 126.1 . .
C6 C10 H10 126.1 . .
Fe C10 H10 126.7 . .
O C11 N 122.0(2) . .
O C11 C1 121.9(2) . .
N C11 C1 116.0(2) . .
C17 C12 C13 118.4(3) . .
C17 C12 P 118.2(2) . .
C13 C12 P 123.3(2) . .
C14 C13 C12 120.7(3) . .
C14 C13 H13 119.6 . .
C12 C13 H13 119.6 . .
C15 C14 C13 120.1(4) . .
C15 C14 H14 120.0 . .
C13 C14 H14 120.0 . .
C14 C15 C16 120.5(3) . .
C14 C15 H15 119.7 . .
C16 C15 H15 119.7 . .
C15 C16 C17 119.6(3) . .
C15 C16 H16 120.2 . .
C17 C16 H16 120.2 . .
C12 C17 C16 120.7(3) . .
C12 C17 H17 119.7 . .
C16 C17 H17 119.7 . .
C19 C18 C23 118.5(2) . .
C19 C18 P 122.1(2) . .
C23 C18 P 119.3(2) . .
C20 C19 C18 120.5(3) . .
C20 C19 H19 119.7 . .
C18 C19 H19 119.7 . .
C21 C20 C19 119.8(3) . .
C21 C20 H20 120.1 . .
C19 C20 H20 120.1 . .
C22 C21 C20 120.5(3) . .
C22 C21 H21 119.7 . .
C20 C21 H21 119.7 . .
C21 C22 C23 119.9(3) . .
C21 C22 H22 120.1 . .
C23 C22 H22 120.1 . .
C22 C23 C18 120.8(3) . .
C22 C23 H23 119.6 . .
C18 C23 H23 119.6 . .
N C24 H24A 109.5 . .
N C24 H24B 109.5 . .
H24A C24 H24B 109.5 . .
N C24 H24C 109.5 . .
H24A C24 H24C 109.5 . .
H24B C24 H24C 109.5 . .
Cl3S C1S Cl1S 124.39(14) . .
Cl3S C1S Cl2S 113.3(3) . .
Cl1S C1S Cl2S 104.47(10) . .
Cl3S C1S H1S 104.3 . .
Cl1S C1S H1S 104.0 . .
Cl2S C1S H1S 104.3 . .
O3A Cl1A O4A 110.8(5) . .
O3A Cl1A O1A 112.0(4) . .
O4A Cl1A O1A 108.6(3) . .
O3A Cl1A O2A 109.8(7) . .
O4A Cl1A O2A 107.1(4) . .
O1A Cl1A O2A 108.4(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ag P 2.4256(6) 2_556
Ag P 2.4256(6) .
Ag O 2.4681(19) .
Ag O 2.4681(19) 2_556
Fe C7 2.028(3) .
Fe C6 2.031(2) .
Fe C1 2.041(3) .
Fe C5 2.042(3) .
Fe C8 2.043(3) .
Fe C3 2.043(3) .
Fe C2 2.045(3) .
Fe C10 2.046(2) .
Fe C9 2.050(3) .
Fe C4 2.051(3) .
P C6 1.793(3) .
P C18 1.826(3) .
P C12 1.829(3) .
O C11 1.231(3) .
N C11 1.337(4) .
N C24 1.446(4) .
N H1N 0.8602 .
C1 C5 1.428(4) .
C1 C2 1.429(4) .
C1 C11 1.481(3) .
C2 C3 1.405(4) .
C2 H2 0.9500 .
C3 C4 1.408(5) .
C3 H3 0.9500 .
C4 C5 1.424(4) .
C4 H4 0.9500 .
C5 H5 0.9500 .
C6 C7 1.431(4) .
C6 C10 1.438(3) .
C7 C8 1.420(4) .
C7 H7 0.9500 .
C8 C9 1.420(4) .
C8 H8 0.9500 .
C9 C10 1.414(4) .
C9 H9 0.9500 .
C10 H10 0.9500 .
C12 C17 1.389(4) .
C12 C13 1.396(4) .
C13 C14 1.388(4) .
C13 H13 0.9500 .
C14 C15 1.368(5) .
C14 H14 0.9500 .
C15 C16 1.382(6) .
C15 H15 0.9500 .
C16 C17 1.396(4) .
C16 H16 0.9500 .
C17 H17 0.9500 .
C18 C19 1.394(4) .
C18 C23 1.397(4) .
C19 C20 1.392(4) .
C19 H19 0.9500 .
C20 C21 1.382(4) .
C20 H20 0.9500 .
C21 C22 1.376(5) .
C21 H21 0.9500 .
C22 C23 1.388(4) .
C22 H22 0.9500 .
C23 H23 0.9500 .
C24 H24A 0.9800 .
C24 H24B 0.9800 .
C24 H24C 0.9800 .
C1S Cl3S 1.547(3) .
C1S Cl1S 1.729(4) .
C1S Cl2S 1.895(5) .
C1S H1S 1.0000 .
Cl1A O3A 1.347(7) .
Cl1A O4A 1.429(5) .
Cl1A O1A 1.433(4) .
Cl1A O2A 1.468(7) .
